#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/56/7035691.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7035691
loop_
_publ_author_name
'Yang, Ting-Hai'
'Silva, Ana Rosa'
'Fu, Lianshe'
'Shi, Fa-Nian'
_publ_section_title
;
 Ionothermal synthesis, crystal structure, topology and catalytic
 properties of heterometallic coordination polymers constructed from
 N-(phosphonomethyl) iminodiacetic acid.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13745
_journal_page_last               13751
_journal_paper_doi               10.1039/c5dt02176f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H42 Dy Fe7 N6 O42 P6, 2(H1.98 O)'
_chemical_formula_sum            'C30 H46 Dy Fe7 N6 O44 P6'
_chemical_formula_weight         1934.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-23 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.2875(5)
_cell_length_b                   15.2875(5)
_cell_length_c                   22.7526(17)
_cell_measurement_reflns_used    1656
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.36
_cell_volume                     4605.1(4)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7855
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_T_max  0.6727
_exptl_absorpt_correction_T_min  0.6389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2874
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2019
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0867P)²+89.0669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                1708
_reflns_number_total             2019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02176f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7035690--7035693.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7035691
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Dy1 Dy 0.6667 0.3333 0.8333 0.0128(2) Uani 1 6 d S
Fe1 Fe 0.89904(8) 0.77519(8) 0.75554(5) 0.0235(3) Uani 1 1 d .
Fe2 Fe 0.6667 0.3333 0.63386(16) 0.0170(7) Uani 0.50 3 d SP
P1 P 0.75627(14) 0.54332(13) 0.72475(8) 0.0173(4) Uani 1 1 d .
N1 N 0.7293(5) 0.6973(5) 0.7627(3) 0.0224(13) Uani 1 1 d .
C1 C 0.6867(6) 0.6113(5) 0.7213(3) 0.0214(15) Uani 1 1 d .
H1A H 0.6898 0.6360 0.6816 0.026 Uiso 1 1 calc R
H1B H 0.6163 0.5657 0.7308 0.026 Uiso 1 1 calc R
C2 C 0.6991(6) 0.6615(6) 0.8239(3) 0.0273(17) Uani 1 1 d .
H2A H 0.6590 0.5884 0.8236 0.033 Uiso 1 1 calc R
H2B H 0.6564 0.6871 0.8384 0.033 Uiso 1 1 calc R
C3 C 0.7852(6) 0.6925(6) 0.8657(3) 0.0268(17) Uani 1 1 d .
C4 C 0.7021(6) 0.7736(6) 0.7462(4) 0.0276(17) Uani 1 1 d .
H4A H 0.6406 0.7595 0.7665 0.033 Uiso 1 1 calc R
H4B H 0.6887 0.7692 0.7043 0.033 Uiso 1 1 calc R
C5 C 0.7862(6) 0.8815(6) 0.7614(3) 0.0241(16) Uani 1 1 d .
O1 O 0.8671(4) 0.6268(4) 0.7350(2) 0.0207(10) Uani 1 1 d .
O2 O 0.7181(4) 0.4695(4) 0.7749(2) 0.0242(11) Uani 1 1 d .
O3 O 0.7432(4) 0.4951(4) 0.6650(2) 0.0283(12) Uani 1 1 d .
O4 O 0.8749(4) 0.7442(5) 0.8506(3) 0.0341(13) Uani 1 1 d .
O5 O 0.7611(5) 0.6633(5) 0.9198(2) 0.0357(14) Uani 1 1 d .
H5 H 0.7004 0.6411 0.9245 0.053 Uiso 1 1 calc R
O6 O 0.8728(4) 0.8969(4) 0.7719(2) 0.0297(13) Uani 1 1 d .
O7 O 0.7615(4) 0.9486(4) 0.7594(3) 0.0304(13) Uani 1 1 d .
O8 O 1.0000 0.0000 1.051(5) 0.62(17) Uani 1 3 d SD
H8A H 1.0182 0.0619 1.0543 0.743 Uiso 0.33 1 d PRD
H8B H 0.9558 -0.0264 1.0244 0.743 Uiso 0.33 1 d PRD
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Dy1 O2 88.78(19) 18_546 17_556
O2 Dy1 O2 180.0(2) 18_546 3_665
O2 Dy1 O2 91.22(19) 17_556 3_665
O2 Dy1 O2 91.22(19) 18_546 2_655
O2 Dy1 O2 179.998(1) 17_556 2_655
O2 Dy1 O2 88.78(19) 3_665 2_655
O2 Dy1 O2 91.22(19) 18_546 .
O2 Dy1 O2 91.22(19) 17_556 .
O2 Dy1 O2 88.78(19) 3_665 .
O2 Dy1 O2 88.78(19) 2_655 .
O2 Dy1 O2 88.78(19) 18_546 16_656
O2 Dy1 O2 88.78(19) 17_556 16_656
O2 Dy1 O2 91.22(19) 3_665 16_656
O2 Dy1 O2 91.22(19) 2_655 16_656
O2 Dy1 O2 179.998(1) . 16_656
O7 Fe1 O1 86.2(2) 2_765 .
O7 Fe1 O6 114.9(2) 2_765 .
O1 Fe1 O6 158.9(2) . .
O7 Fe1 O3 89.8(2) 2_765 13_666
O1 Fe1 O3 99.9(2) . 13_666
O6 Fe1 O3 80.6(2) . 13_666
O7 Fe1 O4 93.5(2) 2_765 .
O1 Fe1 O4 93.5(2) . .
O6 Fe1 O4 86.1(2) . .
O3 Fe1 O4 166.4(2) 13_666 .
O7 Fe1 N1 165.0(2) 2_765 .
O1 Fe1 N1 82.1(2) . .
O6 Fe1 N1 77.2(2) . .
O3 Fe1 N1 101.5(2) 13_666 .
O4 Fe1 N1 77.9(2) . .
O3 Fe2 O3 110.64(16) 3_665 .
O3 Fe2 O3 110.64(16) 3_665 2_655
O3 Fe2 O3 110.64(15) . 2_655
O2 P1 O3 114.2(3) . .
O2 P1 O1 111.0(3) . .
O3 P1 O1 111.2(3) . .
O2 P1 C1 110.0(3) . .
O3 P1 C1 105.4(3) . .
O1 P1 C1 104.3(3) . .
C4 N1 C1 111.6(6) . .
C4 N1 C2 111.9(6) . .
C1 N1 C2 110.7(6) . .
C4 N1 Fe1 105.7(5) . .
C1 N1 Fe1 107.6(4) . .
C2 N1 Fe1 109.1(4) . .
N1 C1 P1 110.8(5) . .
N1 C1 H1A 109.5 . .
P1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
P1 C1 H1B 109.5 . .
H1A C1 H1B 108.1 . .
N1 C2 C3 114.7(6) . .
N1 C2 H2A 108.6 . .
C3 C2 H2A 108.6 . .
N1 C2 H2B 108.6 . .
C3 C2 H2B 108.6 . .
H2A C2 H2B 107.6 . .
O4 C3 O5 121.0(7) . .
O4 C3 C2 122.9(7) . .
O5 C3 C2 116.1(7) . .
N1 C4 C5 112.1(6) . .
N1 C4 H4A 109.2 . .
C5 C4 H4A 109.2 . .
N1 C4 H4B 109.2 . .
C5 C4 H4B 109.2 . .
H4A C4 H4B 107.9 . .
O6 C5 O7 125.2(8) . .
O6 C5 C4 119.0(7) . .
O7 C5 C4 115.7(7) . .
P1 O1 Fe1 119.2(3) . .
P1 O2 Dy1 165.1(3) . .
P1 O3 Fe1 131.2(3) . 13_666
P1 O3 Fe2 133.3(3) . .
Fe1 O3 Fe2 94.6(2) 13_666 .
C3 O4 Fe1 114.9(5) . .
C3 O5 H5 109.5 . .
C5 O6 Fe1 116.7(5) . .
C5 O7 Fe1 118.7(5) . 3_675
H8A O8 H8B 109.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O2 2.254(5) 18_546
Dy1 O2 2.254(5) 17_556
Dy1 O2 2.254(5) 3_665
Dy1 O2 2.254(5) 2_655
Dy1 O2 2.254(5) .
Dy1 O2 2.254(5) 16_656
Fe1 O7 2.103(6) 2_765
Fe1 O1 2.120(5) .
Fe1 O6 2.123(6) .
Fe1 O3 2.154(5) 13_666
Fe1 O4 2.205(6) .
Fe1 N1 2.256(6) .
Fe2 O3 2.257(6) 3_665
Fe2 O3 2.257(6) .
Fe2 O3 2.257(6) 2_655
P1 O2 1.503(5) .
P1 O3 1.512(5) .
P1 O1 1.546(5) .
P1 C1 1.823(7) .
N1 C4 1.470(10) .
N1 C1 1.479(9) .
N1 C2 1.482(9) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.496(11) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 O4 1.240(9) .
C3 O5 1.299(9) .
C4 C5 1.540(11) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 O6 1.246(10) .
C5 O7 1.259(9) .
O3 Fe1 2.154(5) 13_666
O5 H5 0.8200 .
O7 Fe1 2.103(6) 3_675
O8 H8A 0.8454 .
O8 H8B 0.8460 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O1 0.82 1.81 2.555(8) 149.5 18_546
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O7 Fe1 N1 C4 170.9(8) 2_765 .
O1 Fe1 N1 C4 -149.8(5) . .
O6 Fe1 N1 C4 26.1(5) . .
O3 Fe1 N1 C4 -51.3(5) 13_666 .
O4 Fe1 N1 C4 114.8(5) . .
O7 Fe1 N1 C1 -69.7(10) 2_765 .
O1 Fe1 N1 C1 -30.5(4) . .
O6 Fe1 N1 C1 145.4(5) . .
O3 Fe1 N1 C1 68.0(4) 13_666 .
O4 Fe1 N1 C1 -125.9(5) . .
O7 Fe1 N1 C2 50.4(11) 2_765 .
O1 Fe1 N1 C2 89.6(5) . .
O6 Fe1 N1 C2 -94.4(5) . .
O3 Fe1 N1 C2 -171.8(5) 13_666 .
O4 Fe1 N1 C2 -5.7(5) . .
C4 N1 C1 P1 158.8(5) . .
C2 N1 C1 P1 -75.8(7) . .
Fe1 N1 C1 P1 43.3(5) . .
O2 P1 C1 N1 83.0(5) . .
O3 P1 C1 N1 -153.3(5) . .
O1 P1 C1 N1 -36.1(5) . .
C4 N1 C2 C3 -111.5(7) . .
C1 N1 C2 C3 123.3(7) . .
Fe1 N1 C2 C3 5.1(8) . .
N1 C2 C3 O4 0.1(11) . .
N1 C2 C3 O5 179.2(7) . .
C1 N1 C4 C5 -146.3(6) . .
C2 N1 C4 C5 88.9(8) . .
Fe1 N1 C4 C5 -29.7(7) . .
N1 C4 C5 O6 16.5(10) . .
N1 C4 C5 O7 -166.5(6) . .
O2 P1 O1 Fe1 -108.3(3) . .
O3 P1 O1 Fe1 123.3(3) . .
C1 P1 O1 Fe1 10.1(4) . .
O7 Fe1 O1 P1 179.6(3) 2_765 .
O6 Fe1 O1 P1 -2.0(8) . .
O3 Fe1 O1 P1 -91.3(3) 13_666 .
O4 Fe1 O1 P1 86.3(3) . .
N1 Fe1 O1 P1 9.1(3) . .
O3 P1 O2 Dy1 22.6(15) . .
O1 P1 O2 Dy1 -104.1(14) . .
C1 P1 O2 Dy1 141.0(13) . .
O2 Dy1 O2 P1 -159.5(13) 18_546 .
O2 Dy1 O2 P1 111.7(12) 17_556 .
O2 Dy1 O2 P1 20.5(13) 3_665 .
O2 Dy1 O2 P1 -68.3(12) 2_655 .
O2 Dy1 O2 P1 12(10) 16_656 .
O2 P1 O3 Fe1 172.5(4) . 13_666
O1 P1 O3 Fe1 -60.8(5) . 13_666
C1 P1 O3 Fe1 51.6(5) . 13_666
O2 P1 O3 Fe2 5.8(6) . .
O1 P1 O3 Fe2 132.4(4) . .
C1 P1 O3 Fe2 -115.2(4) . .
O3 Fe2 O3 P1 -69.2(4) 3_665 .
O3 Fe2 O3 P1 53.7(5) 2_655 .
O3 Fe2 O3 Fe1 120.7(3) 3_665 13_666
O3 Fe2 O3 Fe1 -116.3(3) 2_655 13_666
O5 C3 O4 Fe1 175.4(6) . .
C2 C3 O4 Fe1 -5.5(10) . .
O7 Fe1 O4 C3 -161.3(6) 2_765 .
O1 Fe1 O4 C3 -74.9(6) . .
O6 Fe1 O4 C3 83.9(6) . .
O3 Fe1 O4 C3 95.2(11) 13_666 .
N1 Fe1 O4 C3 6.2(6) . .
O7 C5 O6 Fe1 -168.1(6) . .
C4 C5 O6 Fe1 8.6(9) . .
O7 Fe1 O6 C5 169.5(5) 2_765 .
O1 Fe1 O6 C5 -8.7(9) . .
O3 Fe1 O6 C5 84.2(5) 13_666 .
O4 Fe1 O6 C5 -98.4(6) . .
N1 Fe1 O6 C5 -20.0(5) . .
O6 C5 O7 Fe1 13.9(10) . 3_675
C4 C5 O7 Fe1 -162.9(5) . 3_675
